EP1695038B1 - Steuerung des flusses von aus feststoffen sublimierten dämpfen - Google Patents

Steuerung des flusses von aus feststoffen sublimierten dämpfen Download PDF

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Publication number
EP1695038B1
EP1695038B1 EP20040813385 EP04813385A EP1695038B1 EP 1695038 B1 EP1695038 B1 EP 1695038B1 EP 20040813385 EP20040813385 EP 20040813385 EP 04813385 A EP04813385 A EP 04813385A EP 1695038 B1 EP1695038 B1 EP 1695038B1
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EP
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Prior art keywords
vapor
throttle valve
vaporizer
temperature
pressure
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English (en)
French (fr)
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EP1695038A2 (de
EP1695038A4 (de
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Thomas N. Horsky
Robert W. Milgate, Iii.
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Semequip Inc
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Semequip Inc
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/26—Bombardment with radiation
    • H01L21/263—Bombardment with radiation with high-energy radiation
    • H01L21/265—Bombardment with radiation with high-energy radiation producing ion implantation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/30—Electron-beam or ion-beam tubes for localised treatment of objects
    • H01J37/317—Electron-beam or ion-beam tubes for localised treatment of objects for changing properties of the objects or for applying thin layers thereon, e.g. for ion implantation
    • H01J37/3171—Electron-beam or ion-beam tubes for localised treatment of objects for changing properties of the objects or for applying thin layers thereon, e.g. for ion implantation for ion implantation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/48—Ion implantation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C23C14/564—Means for minimising impurities in the coating chamber such as dust, moisture, residual gases
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J27/00—Ion beam tubes
    • H01J27/02—Ion sources; Ion guns
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J27/00—Ion beam tubes
    • H01J27/02—Ion sources; Ion guns
    • H01J27/022—Details
    • H01J27/024—Extraction optics, e.g. grids
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/04—Arrangements of electrodes and associated parts for generating or controlling the discharge, e.g. electron-optical arrangement, ion-optical arrangement
    • H01J37/08—Ion sources; Ion guns
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/38—Exhausting, degassing, filling, or cleaning vessels
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2209/00—Apparatus and processes for manufacture of discharge tubes
    • H01J2209/01—Generalised techniques
    • H01J2209/017—Cleaning
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/006—Details of gas supplies, e.g. in an ion source, to a beam line, to a specimen or to a workpiece
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/02—Details
    • H01J2237/022—Avoiding or removing foreign or contaminating particles, debris or deposits on sample or tube
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/0318—Processes
    • Y10T137/0324—With control of flow by a condition or characteristic of a fluid
    • Y10T137/0357—For producing uniform flow
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/7722—Line condition change responsive valves
    • Y10T137/7758—Pilot or servo controlled
    • Y10T137/7759—Responsive to change in rate of fluid flow
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/7722—Line condition change responsive valves
    • Y10T137/7758—Pilot or servo controlled
    • Y10T137/7759—Responsive to change in rate of fluid flow
    • Y10T137/776—Control by pressures across flow line valve
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/7722—Line condition change responsive valves
    • Y10T137/7758—Pilot or servo controlled
    • Y10T137/7761—Electrically actuated valve
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/8593—Systems
    • Y10T137/85954—Closed circulating system
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/8593—Systems
    • Y10T137/85978—With pump
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/8593—Systems
    • Y10T137/85978—With pump
    • Y10T137/85986—Pumped fluid control
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/8593—Systems
    • Y10T137/85978—With pump
    • Y10T137/85986—Pumped fluid control
    • Y10T137/86002—Fluid pressure responsive

Definitions

  • This invention relates to the controlled sublimation of solid materials under vacuum combined with accurate control of flow of the produced vapor to a vacuum chamber with little pressure drop.
  • An important application is the controlled feed of vapor into the evacuated ionization chamber of an ion source for producing an ion beam.
  • the beam may be used for ion implantation into semiconductor substrates.
  • Another important application is the controlled flow of vapor into a vacuum processing chamber for interaction with a work piece.
  • the ionization chamber of an ion source functions under vacuum and requires the material that is to be ionized to be fed in gaseous form with great accuracy and reproducibility.
  • Solids of interest typically have low vapor pressure and must first be sublimated through heating in a reduced pressure environment to produce a volume of vapor. This vapor must then be introduced into the vacuum chamber at the flow, or number of molecules per second, required by the operation to be conducted in the chamber. Since this flow requirement is similar to that required for the introduction of normal gases, standard gas handling equipment has been used for delivery of solid-derived vapor, but with mixed success.
  • the gas source is held at a pressure P 0 substantially higher than the inlet delivery pressure, P D , for the vacuum chamber.
  • P D In order to accurately control the flow of gas into the vacuum chamber, P D must be accurately controlled. This is usually accomplished by a commercially available mass flow controller (MFC) located between the gas source and vacuum chamber inlet.
  • MFC mass flow controller
  • An MFC is a digitally controlled device which varies its conductance to match the delivered mass flow (in grams per second) with the requested mass flow, in a closed-loop manner. Since MFC's are commonly used with relatively high pressure gas sources, MFC's are commonly constructed to operate in a range of correspondingly small conductances, which establish relatively large pressure drops. For vaporized solid materials such as the borohydride decaborane (B 10 H 14 ) or octadecaborane (B 18 H 22 ), this approach suffers from several serious problems.
  • the vapors are derived from a fixed solid charge.
  • the material of the charge is placed in the vaporizer in powder form.
  • the vaporizing area of the fixed charge diminishes over time as the charge is consumed, and especially when the solid materials are susceptible to molecular disassociation if temperatures become too high. Serious problems arise especially when the operation in which the vapors are to be employed requires accurate maintenance of vapor flow, which is often the case.
  • US2003/0072875 A1 discloses a vaporizer connected to a vacuum chamber via a flow monitor with a pressure sensor. The flow measurement is fed to a controller and used to regulate the temperature of the upstream vaporizer and thereby the upstream pressure.
  • SULLIVAN J J ET AL "MASS FLOW MEASUREMENT AND CONTROL OF LOW VAPOR PRESSURE SOURCES” JOURNAL OF VACUUM SCIENCE AND TECHNOLOGY: PART A, AVS /AIP, MELVILLE, NY.; US, vol. 7, no. 3, PART 02, 1 May 1989, pages 2387-2392, ISSN: 0734-2101 discloses a vaporizer and control of a downstream throttle valve by the use of a pressure sensor downstream of the throttle valve.
  • the present invention relates to a vapor delivery system according to claim 1 and to the use of the vapor delivery system for sublimation of solid material according to claims 13 and 14.
  • FIG. 1A is a diagram of an ion source 10.
  • the details of its construction, as well as its preferred modes of ionizing action, are disclosed in detail by Horsky et al., WO2004/003973 filed June 26, 2003 : "An ion implantation device and a method of semiconductor manufacturing by the implantation of boron hydride cluster ions", and by Horsky, U.S. Patent No. US 2004 000647 171 , "Electron impact ion source", filed June 26, 2002, U.S. Patent 6,686,595 , each herein incorporated by reference.
  • the ion source 10 is made to interface to an evacuated vacuum chamber of an ion implanter by way of a mounting flange 36.
  • the portion of the ion source 10 to the right of flange 36, shown in FIG. 1A is under a high vacuum (pressure ⁇ 1x10 -4 Torr).
  • the ion source is maintained at an elevated voltage by a high voltage power supply and is electrically isolated from remaining portions of the high vacuum housing.
  • Gaseous material is introduced into ionization chamber 44 in which the gas molecules are ionized by electron impact from electron beam 70A or 70B.
  • the electron beam exits ionization chamber 44 through the opposite aperture 71B or 71A, or may be absorbed by a beam dump or walls of the chamber acting as a beam dump.
  • a single electron gun and a beam dump shown in FIG.
  • the electron beam originates from a cathode in the electron gun 112, is bent by a magnetic field 135 produced by magnet 130 and pole pieces 125, and enters the ionization chamber 44 through electron entrance aperture 71A or 71B such that electron beam 70A or 70B moves parallel to an elongated ion extraction aperture 81.
  • the electron beam 70 is stopped by beam dump 72 located external to ionization chamber 44.
  • beam dump 72 located external to ionization chamber 44.
  • ions are created adjacent to the ion extraction aperture 81, which appears as a slot in the ion extraction aperture plate 80.
  • the ions are then extracted and formed into an energetic ion beam by an extraction electrode (not shown) located in front of the ion extraction aperture plate 80, and held at a substantially lower voltage.
  • gases may be fed into the ionization chamber 44 via a gas conduit 33.
  • Solid feed materials such as decaborane and octadecaborane can be vaporized in vaporizer 28, and the vapor fed into the ionization chamber 44 through vapor conduit 32 within the source block 35.
  • ionization chamber 44, ion extraction aperture 80, source block 35 (including vapor feed conduit 32), and vaporizer housing 30 are all fabricated of aluminum.
  • Solid feed material 29, located under a perforated separation barrier 34a, is held at a uniform temperature by closed-loop temperature control of the vaporizer housing 30.
  • Sublimated vapor 50 which accumulates in a ballast volume 31 feeds through conduit 39 and through throttling valve 100 and shutoff valve 110.
  • the nominal pressure of vapor 50 between throttling valve 100 and shutoff valve 110 is monitored by capacitance manometer gauge 60.
  • the vapor 50 feeds into the ionization chamber 44 through a vapor conduit 32, located in the source block 35.
  • both gaseous and vaporized materials may be ionized by this ion source.
  • the flow of vapor to ionization chamber 44 is determined by the vapor pressure in the region just before vapor feed conduit 32, i.e., within shutoff valve 110. This is measured by a capacitance manometer pressure gauge 60 located between throttling valve 100 and shutoff valve 110. In general, the flow rate is proportional to the vapor pressure. This allows the pressure signal to represent flow, and to be used as a set-point to select flow.
  • vaporizer housing 30 is brought to a temperature such that when throttling valve 100 is in its fully open position, the desired flow rate is exceeded. Then the throttling valve 100 is adjusted to reach the desired pressure output.
  • the particular ion source shown is an electron-impact ion source which is fully temperature-controlled. Instead of striking an arc-discharge plasma to create ions, this ion source uses a "soft" electron-impact ionization of the process gas by energetic electrons injected in the form of one or more focused electron beams. The "soft" ionization process preserves the large molecules so that ionized clusters are formed. As seen in FIG. 1A and FIG. 1B , solid boron hydride is heated in the vaporizer and flowed through the vapor conduit to a metal chamber, i.e., the ionization chamber.
  • An electron gun located external to the ionization chamber delivers a high-current stream of energetic electrons into the ionization chamber; this electron stream is directed roughly parallel and adjacent to an extended slot in the front of the chamber. Ions are extracted from this slot by an ion extraction electrode, forming an energetic ion beam.
  • an ion extraction electrode located external to the ionization chamber
  • all surfaces are held at a higher temperature than that of the vaporizer (but well below the temperature of dissociation), to prevent condensation of the vapor. Over many hours of testing, we have confirmed that the surfaces of the vapor feed and valves indeed, remain clean.
  • FIGs. 7E , F and G respectively illustrate a gate valve closed, opened a first amount and opened a second, greater amount, functioning as a high maximum conductance throttle valve.
  • a vapor delivery system for delivering a steady flow of sublimated vapor to a vacuum chamber 130.
  • the vacuum chamber may be an ionization chamber having a different ionizing action than that described above, or may be a vacuum processing chamber in which the vapor interacts with other material.
  • the vapor delivery system is comprised of a vaporizer 28, a mechanical throttling valve 100, and a pressure gauge 60.
  • the vapor flow rate is determined by both the temperature of the vaporizer 28 and the conductance of the mechanical throttle valve 100 located between the vaporizer and the inlet conduit 32 to the vacuum chamber.
  • the temperature of the vaporizer 28 is determined by closed-loop control 35 to a set-point temperature.
  • the mechanical throttle valve 100 is electrically controlled, i.e. the valve position is under closed-loop control 120 to the output of the pressure gauge.
  • the vapor flow rate may be held proportional to the pressure gauge output.
  • the vapor delivery system described meets the challenges inherent in delivering a controlled vapor flow over many hours into a vacuum system, e.g. into the ionization chamber of an ion source or more generally, to an operation performed in a vacuum chamber.
  • the system enables certain rules to be observed, which offer significant advantages over prior systems, especially when using low-temperature materials such as decaborane or octadecaborane:
  • the form of the closed loop-controlled, pressure based system intended to deliver sublimed, gas phase material into a vacuum chamber with continuous pumping obeys well-defined laws.
  • solid material 29 is vaporized to vapors 50 contained in reservoir 31.
  • the vapors exit reservoir 31 through vaporizer outlet 39, creating a vapor pressure in advance of a throttle (or "throttling") valve 100.
  • throttle valve 100 a pressure gauge (or sensor) 60 followed by a relatively flow-restricting vapor conduit 32 which represents a flow restriction leading to the vacuum chamber.
  • Throttle valve 100 and pressure sensor 60 in combination with a closed-loop controller 120, provide means to control the pressure beyond throttle valve 100 (before conduit 32) by closed-loop control of the throttle valve conductance.
  • the degree the throttle valve 100 is open (valve position) is actively set in real-time by closing the loop on the pressure sensor output, thus servoing the valve position to a downstream pressure set-point.
  • the rate of vapor flow into the vacuum chamber 130 is determined by this downstream pressure and the conductance of vapor outlet conduit 32.
  • Conduit 32 under common nomenclature is characterized as the "metering section" of the flow control system. Conduit 32 introduces vapor into vacuum chamber 130, while vacuum of desired value is maintained in vacuum chamber 130 by vacuum pump 135.
  • the basic gas dynamic requirement for flow in such a system is that the gas phase pressure of the substance to be controlled is higher in the vapor reservoir 31 than it is in the vacuum chamber 130.
  • Pressure-based mass flow control is implemented in such a system by considering the basic equations governing flow in vacuum systems.
  • the simplest case to model is the case of molecular flow, where the mean free path of the gas molecules is large with respect to the physical dimensions of the vacuum system.
  • the molecular flow regime is appropriate to describe the vapor flow into ion implantation systems, for example, using the system of the present invention where the pressure anywhere in the vapor path is ⁇ 1 Torr.
  • the mass flow rate between any two points can be calculated if the pressure P at each of the two points of interest and the conductance C between the two points is known.
  • This equation can be used to estimate the appropriate maximum conductance of the throttling valve to achieve a desired dynamic range for the delivery system.
  • a ratio of C ThrottlingValveMax to C MeteringLength of at least about 5:1 1 or even 10:1 1 or higher is advantageous to maximize vapor flow dynamic range for a given metering length conductance.
  • FIG. 3 shows, in cross section, an ion source appropriate for creating decaborane or octadecaborane ions in an ion implanter. It differs from FIGs. 1A and 1B in depicting a butterfly-type of mechanical throttle valve 100' rather than using a gate valve 100 as the throttle valve as shown in FIG. 1A .
  • the movable element is a circular flow-obstructing disc of size closely fitting a cylindrical passage, and mounted to be rotated about a diameter of the disc that lies perpendicular to the axis of the passage. It presents a vapor path of controlled conductance, see FIGs. 7A, 7B and 7C .
  • the vapor path from vaporizer to ionization chamber is clearly shown.
  • the vapor conduit 150 of FIG. 3 performs the same function as the vapor conduit (metering section) 32 of FIGs. 1 , 1A and 1B .
  • solid borohydride material 140 such as decaborane or octadecaborane, for example
  • vaporizer 145 is heated by vaporizer 145 to sublimate vapor 165 which passes through vaporizer exit port 155, through butterfly-type throttle valve 100', through isolation valve 160, through vapor conduit 150, and into ionization chamber 170 where vapors are ionized by electron beam 175.
  • An extraction electrode (not shown) at an electric potential much different from that of the ion source extracts and forms an ion beam 180 through a vertical slot 185 in the front plate 190 of the ionization chamber 170.
  • FIG. 4 illustrates, in greater detail, one embodiment designed to provide vapor flow into a vacuum chamber 260 to a point of utilization 270.
  • a vacuum process may be conducted, for example, a chemical vapor deposition (CVD) process or low-pressure CVD (LPCVD) process, or other process where thin films are deposited on a work piece, for example boron-containing thin films such as boron nitride.
  • Solid feed material 200 residing in vaporizer 205 is held at a well-defined temperature by heating vaporizer housing 210 to a temperature T above room temperature. Resistive heaters contained within vaporizer housing 210 are actively controlled by vaporizer heater control 215 within a digital vapor feed controller 220.
  • Vaporizer heater control 215 incorporates a closed-loop PID controller (such as an Omron model E5CK-AA1-500, for example), which accepts a set-point temperature from digital vapor feed controller 220 and closes the loop on the temperature readback provided by a thermocouple (TC) output 225 embedded in vaporizer housing 210, and provides variable power 248 to the resistive heaters, for example in the form of a pulse width-modulated heater voltage.
  • Vapors produced from the feed material 200 pass through vaporizer outlet 230 upstream of throttle valve 235.
  • the purpose of throttle valve 235 is to reduce the vapor flow downstream of the valve such that pressure gauge 240 reaches a particular set-point pressure value.
  • This set-point pressure value is provided by digital vapor feed controller 220 to a closed-loop throttle valve position control 245, which servos throttle valve 235 to a mechanical position (by sending a position signal 247 to a motor incorporated into the throttle valve assembly), in which the gauge output 250 equals the set-point value, i.e., the throttle valve position control 245 closes the loop on gauge output 250.
  • the two set-point values, heater set-point value and pressure set-point value are provided to digital vapor feed controller 220 either manually through a user interface, or by coded recipes which provide increased automation capability.
  • throttle valve 235 comprises a butterfly valve, such as a Nor-Cal model 040411-4
  • a throttle valve position control such as provided by Nor-Cal model APC-200-A may be used. All surfaces with which the vapors come in contact are heated at least to the vaporizer temperature, or somewhat higher. Thus, throttle valve 235 and pressure gauge 240 are heated, as well as the passage walls, including those of metering section 232.
  • a temperature of between 100C and 150C is adequate to prevent condensation of feed materials typically used in vaporizer 205.
  • Typical vaporizer temperatures when running decaborane in the configuration shown in FIG. 4 is in the range 25C to 40C, while for octadecaborane it is between 80C and 120C, for example.
  • a heated capacitance manometer such as an MKS Baratron model 628B-22597 or 631A-25845 may be used as pressure gauge 240.
  • a gauge can read pressures in the range of a few milliTorr to a few Torr, and are appropriate for this application.
  • gauges configured from the manufacturer to read a maximum pressure (full scale reading) of either 100mTorr or 500mTorr can be used.
  • Such pressure limits are selected to provide excellent signal-to-noise for control gauge readings of between 20 mTorr and about 100 mTorr (signals near the bottom of range tend to be noisy, potentially making the servo loop less stable).
  • the appropriate set-point pressure value is determined by the desired partial pressure of vapors in vacuum chamber 260, and the vapor conductance between throttle valve 235 and vacuum chamber 260.
  • FIG. 5 shows a process in which vapor flow 227 impinges on a semiconductor work piece 280, in a vacuum environment.
  • a process might be a thin film-deposition process, for example the production of polysilicon films or silicon-germanium films, in which dopant-containing vapors allow P-type or N-type doping of the semiconductor films during film growth.
  • Another important application is plasma doping (PLAD).
  • PLAD plasma doping
  • the substrate is held on a platen electrically isolated from the vacuum chamber, dopant vapors are introduced and a plasma is formed adjacent the platen.
  • One or more high voltage pulses are applied to the platen, and hence the substrate, causing energetic ions of the plasma to be attracted to dope the substrate.
  • FIG. 6 shows a system in which vapor is fed into an ion source for forming an ion beam to perform ion implantation.
  • Vapors pass through throttle valve 235, through vapor conduit 228 of ion source 285 and into the ionization chamber 287 of ion source 285.
  • the ionization chamber 287 is held at high voltage.
  • the vapor is ionized within ionization chamber 287 by an appropriate energizing means; once ions are created, they are extracted into an evacuated chamber, accelerated and formed into an energetic ion beam 295 by extraction optic 290, which is at a substantially different voltage from that of the ionization chamber.
  • the ion beam is directed into an implantation chamber to implant a semiconductor substrate 298 for doping.
  • the process can be the ion implantation into polysilicon coatings on large glass panels for making flat panel displays (FPD doping), for example.
  • the ion beams produced by such systems may be mass analyzed, but frequently have no mass analysis.
  • the ion source is typically quite large, its ionization chamber having one dimension somewhat larger than the shorter dimension of a panel being implemented, which can be a meter long or greater.
  • a stationary "ribbon" beam of ions is extracted from the ion source and focused onto the flat panel, while the panel is mechanically scanned across the beam along the longer dimension of the panel. This process is important in fabricating FPD's which have CMOS driver circuitry along the periphery of the display panels, for example in making thin film transistor-based televisions or computer monitors.
  • FIG. 7 shows a system adapted to the case of a conventional beamline ion implanter having mass analysis.
  • the beam passes into a dispersive dipole electromagnet which separates the unresolved beam 295 into beamlets separated in space according to the mass-to-charge ratio of the ions, as is known in the art.
  • the electromagnet current, and hence the bending, dispersive dipole field can be adjusted so that only ions of a particular mass-to-charge ratio (or a certain preferred range of mass-to-charge ratios, depending on the width of resolving aperture 297) are passed to the semiconductor substrate by resolving aperture 297.
  • the ionization chamber 287 For implanting ions into a semiconductor wafer (e.g. a silicon crystal) the ionization chamber 287 has a volume less than about 100 ml and the maximum flow of sublimated vapor into the chamber is of the order of 1sccm.
  • FIGs. 7A-7C illustrates, in qualitative manner, relative positions of the butterfly valve roughly corresponding as follows: in FIG. 7A : closed position; FIG. 7B : 7.5 degree rotation; FIG. 7C : 15 degree rotation.
  • the rotary positions are controlled electrically by a rotary stepper motor. Clearances between the periphery of rotatable circular plate B of the butterfly and its cylindrical housing H are indicated by C ⁇ C' ⁇ C", where C is the minimum clearance in the "closed" position, of a few thousands of an inch.
  • FIG. 7D shows calculated N 2 conductance as a function of rotation angle for a circular butterfly of 1.4 inch diameter. The points corresponding to FIGs 7A-7C are marked on the curve of FIG. 7D , and are approximately equal to ⁇ 0 l/s, 2 l/s, and 8 l/s, respectively.
  • FIGs. 7E-7G illustrate, in qualitative manner, relative positions of a sliding gate valve implemented as a throttle valve, see FIGs. 1A and 1B . Shown are: FIG. 7E : gate G in closed position; FIG. 7F : gate G 10% open; FIG. 7G : 30% open.
  • the gate valve available in a variety of diameters from about 0.5 inch to 2.5 inches, functions as both a shutoff valve (seals when closed) and a throttle valve (with a stepper motor operating the valve actuator).
  • the butterfly valve is not a sealing valve; i.e., it has a small but finite conductance when closed.
  • FIGs. 8 and 8A show two views of a preferred embodiment of a vapor delivery system for providing vapors to the ion source of an ion implanter, for example the source of FIG. 3 .
  • the overall length of the valve chain is minimized, and is designed to be close-coupled to the ion source. Shown is vaporizer 400, vaporizer isolation valve V1, 410, valve actuator 415, evacuation port 420 (connects to V3, not shown), throttle valve TV1, 430, throttle valve motorized actuator 435, ion source isolation valve V2, 440, V2 actuator 445, heated capacitance gauge G1, 450, N 2 vent valve V4, 460.
  • FIG. 9 shows a schematic of the vapor delivery system of FIG. 8 , indicating the salient control points.
  • the vapor delivery system is depicted controlled through an operator interface 700, through which the operator can provide inputs to open or close valves V1, 410 (vaporizer isolation valve), V2, 440 (ion source isolation valve), V3, 441 (roughing vacuum valve), V4, 460 (vent valve), and TV1 430 (throttle valve); all of these valves provide readbacks to the operator interface to confirm the valve states.
  • V3 is located between the two isolation valves V1 and V2, and is opened when it is necessary to evacuate the dead volume between these two valves, for example after the vaporizer 400 has been removed (with V1) for service or refill and replaced.
  • V4 is used to vent this dead volume to prepare for component removal, for example removal of the vaporizer 400.
  • Other user-accessible inputs include three temperature setpoints: PID 1 for the vaporizer 400, PID 3 for valves V1-V4 and TV1, and a temperature set-point for the ion source block containing the vapor conduit 150 of FIG. 3 .
  • PID 1 for the vaporizer 400
  • PID 3 for valves V1-V4 and TV1
  • a temperature set-point for the ion source block containing the vapor conduit 150 of FIG. 3 In general, all surfaces with which the vapor comes in contact are maintained at a temperature at least as high as that of the vaporizer. It is preferable to maintain ion source set-point temp > PID 3 > PID 1. Via the ion source block, the surfaces of conduit 150 are thus preferably maintained at temperature greater than the set-point of PID 3.
  • PID 2 is a closed-loop controller which adjusts the position of the throttle TV1, 430 to bring the pressure read by pressure gauge G1, 450 to its set-point value.
  • This pressure set-point for the heated pressure gauge G1, 450 reads back to the Operator Interface.
  • This pressure readback signal indicates the vapor pressure between throttle valve TV2 and the vapor conduit to the ion source (vapor conduit 150 in FIG. 3 ), providing the control signal for the closed-loop control of TV1 position.
  • FIG. 10 is a plot of decaborane vapor flow into the ion source of FIG. 3 using the vapor delivery system of FIG. 9 .
  • the butterfly-type throttle valve positions outlined in FIGs. 7A, 7B, 7C are shown on the curve of FIG. 9 .
  • the useful dynamic range of the vapor delivery system covers about a factor of 10, from about 0.1 sccm (standard cc's per minute) to over 1.0 sccm for a vaporizer temperature of 30C, which delivers a fixed vapor pressure upstream of the throttle valve. To obtain higher flows, a higher vaporizer temperature is used.
  • Typical gas flow rates consumed by ion sources for ion implanters are about 2 sccm or less.
  • the vapor delivery conductances and pressures are tuned to the required vapor flows, and to the conductance of the ion source inlet, as shown in FIG. 2 and accompanying text, and will be further expanded in a discussion of FIG. 12 .
  • FIG. 11 shows the response of the control pressure gauge 450 to throttle valve rotation in the system exemplified by FIGs. 3 and 8-10 .
  • the vapor pressure within ionization chamber 170 at about 40 mTorr gauge pressure i.e., pressure at the inlet to the ion source
  • the pressure upstream of the throttle valve is about 65 milliTorr.
  • the greatest pressure drop is across the vapor conduit 150 of the ion source of FIG. 3 , which for the example has an N 2 conductance of about 0.5 l/s.
  • FIG. 12 plots the effective N 2 conductance of the entire vapor delivery chain of FIGs. 3 and 8-10 as a function of rotation angle of a butterfly-type throttle valve.
  • the conductance dynamic range of the throttle valve should be matched to the smallest conductance of the system, in this case the conductance of the conduit 150 into the ion source.
  • the vapor conduit 150 of FIG. 3 for the example is a cylindrical bore about 1 cm in diameter and 25 cm long.
  • a respectively larger or smaller throttle valve (one with a respectively larger or smaller conductance over its dynamic range) should be used.
  • the vapor delivery system herein disclosed enables use of "open" valve and passage structures (high conductances) which are not easily clogged by condensed vapors.
  • all the valves and connecting elements are readily held at a temperature greater than the vaporizer temperature.
  • the vaporizer is maintained at 30C, V1-V4 and TV1 are at 50C, gauge G1 is at 100C, and the ion source is held at >50C. This "staging" of the temperatures of successive elements down the chain prevents any significant condensation of sublimed vapors.
  • the use of high-conductance elements following the vaporizer minimizes the vapor pressure and hence the vaporizer temperature required to reach and sustain the desired flow rates. This increases the useful life of the borohydride or other solid feed materials stored in the vaporizer, since they are known to dissociate or polymerize at elevated temperatures with reactions that are a strong function of temperature.
  • the maximum N 2 gas conductance of the throttle valve is at least 1 liter per second or greater, and the pressure drop across the throttling valve when the valve is fully open is less than 100mTorr, in preferred cases often less than 25mTorr.
  • FIG. 13 shows the time signature of the vapor delivery system when operated in its normal "closed-loop” mode.
  • a pressure set-point is provided by digital vapor feed controller 220 to throttle valve position control 245.
  • the position control adjusts the valve position to minimize the "error" between control gauge output 250 and the pressure set-point value. This is accomplished by a so-called PID (Proportional Integral Differential) control loop which can be programmed to have well-defined response characteristics such as speed and settling time, and degree of overshoot, for example.
  • PID Proportional Integral Differential
  • the Nor-Cal model APC-200-A incorporates such a PID controller, coupled to a stepper motor which turns the shaft to which the circular plate of the butterfly throttle valve is mounted.
  • a stepper motor which turns the shaft to which the circular plate of the butterfly throttle valve is mounted.
  • FIG. 13 shows the rapid settling time and excellent reproducibility of this system when using octadecaborane (B 18 H 22 ) feed material.
  • SP1 set-point
  • SP2 set-point
  • FIG. 14 illustrates a remote implementation of the vapor delivery system of FIGs. 4-7 , for example the vaporizer, throttle valve, and other flow control elements are located in the gas distribution box of an ion implanter, requiring a connecting tube of up to a meter long to connect to the inlet to the ion source.
  • the overall conductance of the vapor delivery chain is not significantly reduced, and remains dominated by the ion source's vapor inlet conductance in accordance with FIG. 2 .
  • FIG. 15 illustrates further important feature of the vapor delivery system. It is known that the rate at which feed material vaporizes is a function of its open surface area, particularly the available surface area at the solid-vacuum interface. As feed material in powder form within the vaporizer is consumed over time, this available surface area steadily decreases, resulting in a decrease in the vapor pressure preceding the throttle valve until the evolution rate of vapors cannot support the desired vapor flow rate. This is known as “evolution rate limited" operation.
  • a vaporizer temperature of, say, 25C might support the required vapor flow at a nominal throttle valve position at the low end of its dynamic range, for example that represented by point 7B indicated on the curve of FIG.
  • a valve position commensurate with point 7C indicated on the curve of FIG. 10 might then be necessary to maintain the same desired flow.
  • the state of the system is now such that the throttle valve is near the high displacement limit of its dynamic range.
  • this displacement is sensed by the vapor feed controller 220. It sends a new, higher heater set-point temperature as by signal 246, FIG. 14 , to vaporizer heater control (or regulator) 215.
  • the vapor feed controller possesses resident lookup table information which determines the next incremental temperature change that would produce a desired increase of vapor generation and pressure increase preceding the throttle valve. For example, for nominal 30C operation, the next increment could be 2C, a change to 32C.
  • the increment is selected to restore, once the vaporizer temperature settles to its new value, the nominal throttle valve operating point to 7B of FIG. 10 , near the low displacement end of its dynamic range.

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Claims (14)

  1. Dampfzuführungssystem zum Zuführen eines kontrollierten Stromes von aus einem Feststoff (29; 140; 200) sublimiertem Dampf zu einer Vakuumkammer (130; 258; 260), mit der Kombination eines bei subatmosphärischem Druck zu betreibenden beheizten Vaporisators (28; 145; 205; 400) zum Aufnehmen des Feststoffs, der einen Temperaturregler (35) zum Regeln der Temperatur des Vaporisators (28; 145; 205; 400) aufweist, und eines Dampfzuführungskanals (37; 237) von dem Vaporisator zu der Vakuumkammer, wobei der Dampfzuführungskanal ein Drosselventil (100; 100'; 235; 430) und daran anschließend eine Dampfleitung (32; 150; 228) aufweist,
    einem Druckmesser (60; 240; 450), der auf subatmosphärischen Druck anspricht und sich zwischen dem Drosselventil und der Dampfleitung befindet, und wobei ein Regelsystem (60; 120; 240, 250, 245; PID2), das den Druckmesser aufweist, so konstruiert ist, dass es die Konduktanz des Drosselventils verändert, um den subatmosphärischen Druck des Dampfes stromabwärts von dem Drosselventil in Reaktion auf den Ausgang des Druckmessers zu regeln, wobei dadurch der Strom von Dampf zu der Vakuumkammer durch den Druck des Dampfes im Bereich des Kanals zwischen dem Drosselventil und der Dampfleitung (32; 150; 228) bestimmt wird,
    dadurch gekennzeichnet, dass
    Flächen des Dampfzuführungskanals, die dem sublimierten Dampf ausgesetzt sind, einschließlich solcher Flächen des Drosselventils, des Druckmessers und der Dampfleitung, dazu ausgelegt sind, auf einer Temperatur über der Kondensationstemperatur des Feststoffs gehalten zu werden, und dass
    das Regelsystem (60; 120; 240, 250, 245; PID2) dazu ausgelegt ist, die Stellung des Drosselventils (100; 100'; 235; 42) zu überwachen und, wenn sich das Drosselventil (100; 100'; 235; 43) seiner maximal nutzbaren Konduktanz nähert, die Temperatur des Vaporisators (28; 145; 205; 400) zu erhöhen, um den Druck in dem Vaporisator anzuheben und das Drosselventil (100; 100'; 235; 43) innerhalb seiner bevorzugten Konduktanz arbeiten zu lassen.
  2. Dampfzuführungssystem nach Anspruch 1, mit einem Temperaturregelsystem (35) zum Erhitzen der Flächen des Zuführungskanals (37; 237) auf mindestens die Temperatur des Vaporisators.
  3. System nach Anspruch 1 oder 2, das dazu ausgelegt ist, die sowohl durch ein Regelsystem (35; 225, 215, 248; PID1) für die Temperatur des Vaporisators als auch das Regelsystem (60, 120; 240; 250; 245; PID2) für die Konduktanz des Drosselventils zu bestimmende Dampfströmungsgeschwindigkeit durch Regeln der Stellung des Drosselventils anzupassen.
  4. Dampfzuführungssystem nach einem der vorhergehenden Ansprüche, bei dem das Drosselventil ein Schieberventil mit variabler Stellung ist.
  5. Dampfzuführungssystem nach einem der vorhergehenden Ansprüche, bei dem das Drosselventil vom Typ Ventilklappe ist.
  6. Dampfzuführungssystem nach Anspruch 1 in Kombination mit einem drosselventilbasierten Erfassungs- und Regelsystem, das in der Lage ist, einen Vaporisatorsolltemperaturwert einem Regler einer Vaporisatorheizvorrichtung zu übermitteln, die in der Lage ist, die Vaporisatortemperatur auf dem Sollwert zu halten, wobei in dem Erfassungs- und Regelsystem mindestens ein vorbestimmter Ventilverschiebungswert gespeichert ist, der eine gewünschte Obergrenze für die Konduktanz des Drosselventils repräsentiert, wobei das Erfassungs- und Regelsystem so konstruiert ist, dass es die Stellung des Drosselventils überwacht, und das Erfassungs- und Regelsystem so konstruiert ist, dass es, wenn festgestellt wird, dass das Ventil sich jenem Verschiebungswert nähert oder diesen erreicht, den Solltemperaturwert für den Regler der Heizvorrichtung erhöht (beispielsweise durch den Eingang 246), um eine verstärkte Dampferzeugung und einen erhöhten Dampfdruck stromaufwärts von dem Drosselventil zu bewirken und dadurch zu veranlassen, dass die Regelung des Drosselventils bewirkt, dass das Ventil in eine Stellung mit wesentlich niedrigerer Konduktanz zurückkehrt.
  7. Dampfzuführungssystem nach Anspruch 6, mit einer Referenztabelle vorbestimmter Inkremente des Temperaturanstiegs, die für den Betrieb geeignet sind, wobei das Erfassungs- und Regelsystem nach Feststellung, dass das Ventil sich seinem Verschiebungswert nähert oder diesen erreicht, bewirkt, dass die Vaporisatorsolltemperatur auf die nächste Stufe in der Referenztabelle inkrementiert wird.
  8. Dampfzuführungssystem nach einem der vorhergehenden Ansprüche, das so konstruiert und angeordnet ist, dass ionisierbarer Dampf einer Ionenquelle zugeführt wird.
  9. Dampfzuführungssystem nach Anspruch 8, das so konstruiert und angeordnet ist, dass ionisierbarer Dampf der Ionenquelle eines Ionenimplantationsgeräts zugeführt wird.
  10. Dampfzuführungssystem nach einem der vorhergehenden Ansprüche, das so konstruiert und angeordnet ist, dass Dampf einer Vakuumkammer zur Bearbeitung eines Werkstücks zugeführt wird.
  11. Dampfzuführungssystem nach einem der vorhergehenden Ansprüche, das so konstruiert ist, dass es seinen Dampf zu einem Hochvakuum befördert, wobei das System so konstruiert ist, dass es auf eine Abnahme in dem subatmosphärischen Druck stromabwärts von dem Drosselventil (100; 100'; 235; 430) reagiert, um die Temperatur des Vaporisators (28; 145; 205; 400) zu erhöhen.
  12. Dampfzuführungsystem nach einem der vorhergehenden Ansprüche, bei dem das Regelsystem für das Drosselventil einen Hilfsregelkreis umfasst, der die Stellung des Drosselventils (100; 100'; 235; 430) in Reaktion auf das Ausgangssignal des Druckmessers (60; 240; 450) einstellt, um den stromabwärtigen Dampfdruck an dem Druckmesser auf einem Sollwert zu halten.
  13. Verwendung des Dampfzuführungssystems nach einem der vorhergehenden Ansprüche zum Zuführen eines kontrollierten Stromes von aus einem Feststoff sublimiertem Dampf zu einer Vakuumkammer.
  14. Verwendung des Dampfzuführungssystems nach Anspruch 9 oder 10 zum Zuführen eines kontrollierten ionisierbaren Stromes von aus einem Feststoff sublimiertem Dampf zu einer Ionisationskammer, um die Erzeugung eines lonenstrahls in einer Vakuumkammer durchzuführen.
EP20040813385 2003-12-12 2004-12-09 Steuerung des flusses von aus feststoffen sublimierten dämpfen Not-in-force EP1695038B1 (de)

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EP1695038A2 (de) 2006-08-30
TWI326102B (en) 2010-06-11
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WO2005059942A3 (en) 2005-10-13
JP2007521398A (ja) 2007-08-02
CN1964620B (zh) 2010-07-21
TWI328244B (en) 2010-08-01
EP1695038A4 (de) 2009-05-20
US20070210260A1 (en) 2007-09-13
JP4643588B2 (ja) 2011-03-02
TW200523977A (en) 2005-07-16
KR20060126995A (ko) 2006-12-11
CN1964620A (zh) 2007-05-16
JP4646920B2 (ja) 2011-03-09
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US7820981B2 (en) 2010-10-26
US20070241689A1 (en) 2007-10-18
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US7629590B2 (en) 2009-12-08
KR100883148B1 (ko) 2009-02-10
CN1894763B (zh) 2010-12-08
US7723700B2 (en) 2010-05-25
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WO2005060602A3 (en) 2007-01-04
US20080047607A1 (en) 2008-02-28
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US20080121811A1 (en) 2008-05-29
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